Exfoliation and delamination of Ti3C2Tx MXene with HCl + LiF etchant was investigated. Increasing etching temperature promotes the exfoliation but aggravates the oxidation. Washing the exfoliation products by ethanol significantly enhances the delamination. Flexible and highly-conductive Ti3C2Tx papers with tailored thickness were prepared. The delaminated Ti3C2Tx MXene shows superior properties as anode for LIBs.